CN103449820A - Method for reducing sintering temperature of calcium zirconate microwave dielectric ceramic - Google Patents

Method for reducing sintering temperature of calcium zirconate microwave dielectric ceramic Download PDF

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CN103449820A
CN103449820A CN2013102751015A CN201310275101A CN103449820A CN 103449820 A CN103449820 A CN 103449820A CN 2013102751015 A CN2013102751015 A CN 2013102751015A CN 201310275101 A CN201310275101 A CN 201310275101A CN 103449820 A CN103449820 A CN 103449820A
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calcium zirconate
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sintering
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CN103449820B (en
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李谦
李栋
金彪
黄金亮
顾永军
胡婧雯
孙换
李刚
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Henan University of Science and Technology
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Abstract

The invention discloses a method for reducing sintering temperature of calcium zirconate microwave dielectric ceramic. The method disclosed by the invention is a method in which the sintering temperature of CaZrO3 microwave dielectric ceramic is effectively reduced by adding proper Li2O-B2O3-SiO2 is added as a sintering aid so as to effectively reduce the sintering temperature of CaZrO3 microwave dielectric ceramic, realize electrode cofiring and keep an excellent microwave dielectric property. The method comprises the following steps: 1, preparing the Li2O-B2O3-SiO2 sintering aid; and 2, adding the Li2O-B2O3-SiO2 sintering aid to calcium zirconate base stock, carrying out ball milling, drying, baking, grinding, sieving, molding and sintering to obtain the CaZrO3 microwave dielectric ceramic.

Description

A kind of method that reduces calcium zirconate microwave-medium ceramics sintering temperature
Technical field
The present invention relates in a kind of electronic devices and components field to reduce the method for calcium zirconate microwave-medium ceramics sintering temperature, relate in particular to and a kind ofly with sintering aid, reduce CaZrO 3the method of microwave dielectric ceramic materials sintering temperature.
Background technology
Along with scientific and technical progress, the transformation of social production mode of life, the mankind have entered the information age.In order to meet the further social desirability of microminiaturization of mobile communication equipment, multilayer integrated circuit technology has obtained development rapidly, and multilayer sheet type microwave dielectric ceramic components and parts (monolithic structure device) are the only way which must be passed of realizing this great-leap-forward development.Have monolithic structure microwave-medium ceramics components and parts need microwave dielectric ceramic materials can with metal inner electrode layer (as Pt, Ag, Cu etc.) common sintering under the melting temperature lower than metal of high conductivity commonly used.Yet; from the angle of economic results in society and ecological environmental protection, Ag (fusing point is 961 ℃) or Cu (fusing point is 1064 ℃) cheap metal that use itself has than low melting point are the optimal selection of monolithic structure components and parts electrode layer material as inner electrode layer.In recent years, LTCC (Low Temperature Co-fired Ceramic, LTCC) technology can effectively reduce electronic devices and components size in mobile communcations system, realize that unicircuit has been widely studied concern because of it, so this is also the inevitable direction of microwave dielectric ceramic material components and parts Future Development.
CaZrO 3there is perovskite structure, because it has low-loss, high specific inductivity, can be used for electrical condenser and dielectric resonator under microwave condition.Under traditional process for solid phase synthesis, CaZrO 3dIELECTRIC CONSTANT ε rbe about 30, the quality factor q when frequency f is 5.6GHz is about 3000, temperature frequency coefficient τ f=-26.5ppm/℃.Yet, CaZrO 3sintering temperature usually more than 1550 ℃, far above Ag(960 ℃) or Cu(1084 ℃) fusing point, can not realize that electrode burns altogether, therefore reduce CaZrO 3it is very important that the sintering temperature of material seems.
Summary of the invention
The objective of the invention is in order to solve the problems of the technologies described above the deficiency of existence, provide a kind of by adding appropriate Li 2o-B 2o 3-SiO 2for sintering aid, thereby and carried out a supporting technical process and effectively reduced CaZrO 3the microwave-medium ceramics sintering temperature, realize that electrode burns altogether, and keep the method for excellent microwave dielectric property simultaneously.
The technical solution adopted in the present invention is:
With Li 2o-B 2o 3-SiO 2for sintering aid reduces CaZrO 3the method of microwave-medium ceramics sintering temperature, step is as follows:
Step 1, Li 2o-B 2o 3-SiO 2the preparation of sintering aid, Li 2o, B 2o 3, SiO 2proportioning by 7:1:2 is made compound, puts into nylon ball grinder, presses respectively Li 2o-B 2o 3-SiO 2180 ~ 200% and 150 ~ 160% of compound weight adds zirconia ball and deionized water as ball-milling additive, and in planetary ball mill, ball milling is 8 ~ 12 hours, and rotating speed is 200 ~ 220r/min; By ball milling good mixed slurry as in loft drier 120 ℃ dry 8 hours; Compound after drying is placed in to the agate tank and grinds, the compound after grinding is crossed to 120 mesh standard sieves; Compound after sieving is put into to corundum crucible, then be placed in after retort furnace is heated to 800-950 ℃ with the temperature rise rate of 3 ~ 5 ℃/min and be incubated 30 ~ 60min; Adopt melt pulling method that the melt-mixed material after insulation is placed in to deionized water fast, obtain original Li 2o-B 2o 3-SiO 2frit; Using the pristine glass material that obtains respectively by weight 180 ~ 200% and 150 ~ 160% add zirconia ball and dehydrated alcohol as ball-milling additive, ball milling 60 ~ 90min on Quick ball grinder, carry out fragmentation, rotating speed is 1200r/min; By ball milling good glass paste as in loft drier 120 ℃ dry 8 hours; Frit after drying is placed in to the agate tank and grinds, the compound after grinding is crossed to 200 mesh standard sieves, obtain uniform Li 2o-B 2o 3-SiO 2sintering aid;
In step 2, the calcium zirconate base-material that is 100% at weight part, add 3 ~ 12% the Li that accounts for calcium zirconate base-material gross weight 2o-B 2o 3-SiO 2sintering aid, put into nylon ball grinder, by 180 ~ 200% and 150 ~ 160% of calcium zirconate base-material weight, adds zirconia ball and dehydrated alcohol as ball-milling additive respectively, and in planetary ball mill, ball milling is 8 ~ 12 hours, and rotating speed is 200 ~ 220r/min; By ball milling, good mixed slurry is put into 120 ℃ of oven dry of loft drier 8 hours; Compound after drying is placed in to the agate tank and grinds, the compound after grinding is crossed to 120 mesh standard sieves, obtain uniform CaZrO 3ceramic powder; To in the ceramic powder obtained, add the polyvinyl alcohol that weight percent is 6 ~ 8% to carry out granulation as tackiness agent, cross 60 ~ 80 orders; With tabletting machine compression moulding, be green compact again; The green compact of compression moulding, in 800 ℃ ~ 950 ℃ sintering, are incubated to 2 ~ 4 hours, make CaZrO 3microwave-medium ceramics.
Described Li 2o can use Li 2cO 3substitute.
The pressure of described tabletting machine is 156MPa.
The right cylinder that described green compact are 10mm * 3mm.
At preparation Li 2o-B 2o 3-SiO 2having used melt pulling method during sintering aid, is to be beneficial to the compound of reprocessing in order to adopt controlled technique to prepare.
At preparation Li 2o-B 2o 3-SiO 2carried out twice grinding during sintering aid, and sieved, the purpose of grinding for the first time is the mixing that makes raw material full and uniform, the purpose of grinding for the second time is that large glass block is ground to tiny powder, sieve is in order to make the tiny homogenizing of glass powder, so be more conducive to the generation of active liquid phase in the technical process of postorder, the liquid phase be more conducive between solid phase particles has produced more capillary force, makes ceramic particle generation slippage and rearrangement.
At preparation Li 2o-B 2o 3-SiO 2being placed in during sintering aid after retort furnace is heated to 800-950 ℃ with the temperature rise rate of 3 ~ 5 ℃/min and being incubated 30 ~ 60min, is in order to make each component thermally equivalent, fully reaction.
In step 2, compound has been carried out to twice grinding, oven dry and screening, to merge more abundant for sintering aid and solid phase particles, thereby can make in the stupalith sintering process, the sintering aid added reacts the sintering environment of the active liquid phase produced while having improved pure solid phase ceramic powder particle sintering with solid phase particles, thereby greatly reduces ceramic sintering temperature.
In step 2, will in the ceramic powder obtained, add the polyvinyl alcohol that weight percent is 6 ~ 8% to carry out granulation as tackiness agent, cross 60 ~ 80 orders, purpose is thicker in order to make granularity, has the particle of certain false granularity grating, good fluidity, makes powder be easy to moulding.
In step 2 by the green compact of compression moulding in 800 ℃ ~ 950 ℃ sintering, be incubated 2 ~ 4 hours, purpose is in order to make the liquid phase between solid phase particles produce huge capillary force, make ceramic particle generation slippage and rearrangement, meanwhile, make produced capillary vessel power also can cause the dissolving of ceramic particle-precipitation mass transfer, small-particle dissolves, and macrobead is grown up.
Experiment is found, Li 2o-B 2o 3-SiO 2add-on since 3%, performance index start to optimize, when sintering temperature is 900 ℃, soaking time 3h, Li 2o-B 2o 3-SiO 2add-on while being 9%, performance index the best, specific inductivity is 28, quality factor are 9359GHz, temperature coefficient of resonance frequency is-10ppm/ ℃; Yet, Li 2o-B 2o 3-SiO 2add-on higher than 9% the time, performance index start to successively decrease.
The present invention is by adding Li 2o-B 2o 3-SiO 2regulate CaZrO 3sintering temperature, under the sintering temperature of 900 ℃ with Li 2o-B 2o 3-SiO 2for the sintering agent sintering has synthesized the calcium zirconate microwave-medium ceramics.When specific inductivity and temperature coefficient of resonance frequency remain unchanged substantially, on 1550 ℃ of bases of original sintering temperature, nearly 650 ℃ have been reduced.
Adopt Li 2o-B 2o 3-SiO 2the CaZrO prepared as sintering agent 3pottery, make CaZrO 3pottery has reached low-temperature sintering.Low-temperature sintering is a kind of sintering method of sintering aid (admixture) as transition liquid-phase of usining.In the stupalith sintering process, the sintering aid added reacts the sintering environment of the liquid phase produced while having improved pure solid phase ceramic powder particle sintering with solid phase particles, thereby greatly reduces ceramic sintering temperature.The active liquid phase sintering is in the stupalith sintering process, and the liquid phase between solid phase particles has produced huge capillary force, makes ceramic particle generation slippage and rearrangement, thus the acceleration of sintering process.Meanwhile, the capillary vessel power produced also can cause the dissolving of ceramic particle-precipitation mass transfer, and small-particle dissolves, and macrobead is grown up.Point of contact at solid phase particles, huge capillary force makes solid phase solubleness increase, material just migrates to the low solubility district by the high-dissolvability district, thereby makes the particle of zone of action gradually smooth and adjacent to each other, and on macroscopic view, ceramic body reaches the densification effect because of volumetric shrinkage.Due to Li 2o-B 2o 3-SiO 2it is 377 ℃ that the softening temperature of glass hangs down, therefore at CaZrO 3in the sintering process of pottery, Li 2o-B 2o 3-SiO 2glass has become liquid phase, wet ceramic particle, make ceramic particle fully dissolve in liquid phase, mass transfer mode in sintering process is also by the evaporation of solid state sintering-cohesion, diffusion mass transfer has become the dissolving of liquid phase sintering-precipitation and mobile mass transfer, small-particle is dissolved at the point of contact place, pass through mass transfer in liquid phase, on the free surface of larger particle or particle, deposit, thereby the variation of grain growth and grain shape appears, particle is constantly reset and densification simultaneously, simultaneously because mobile rate of mass transfer is faster than diffusion mass transfer speed, slippage and the rearrangement of ceramic particle have been accelerated, thereby the liquid phase sintering densification rate is high, base substrate can be made in the situation that than the fine and close sintered compact of the much lower acquisition of solid state sintering temperature.
With the existing Li that do not add 2o-B 2o 3-SiO 2the preparation method of sintering agent compares, and under lower sintering temperature, the volume density of pottery obviously increases.
By above preparation method, CaZrO 3the sintering temperature of microwave-medium ceramics is reduced, and dielectric properties are optimized.Sintering temperature can be down to below 900 ℃, dielectric properties: DIELECTRIC CONSTANT ε r=27 ~ 31, quality factor q * f=9067 ~ 10196GHz, temperature coefficient of resonance frequency τ f=-15 ~ 6.7ppm/ ℃.
Embodiment
The following stated embodiment describes the present invention in detail, and in these embodiments, unless otherwise indicated, all umbers and per-cent are all calculated by weight.
Preparation technology's flow process of above embodiment:
Step 1, Li-- 2o-B 2o 3-SiO 2the preparation of sintering aid, Li-- 2o, B 2o 3, SiO 2proportioning by 7:10:2 is made compound, puts into nylon ball grinder, presses respectively Li-- 2o-B 2o 3-SiO 2180 ~ 200% and 150 ~ 160% of compound weight adds zirconia ball and deionized water as ball-milling additive, and in planetary ball mill, ball milling is 8 ~ 12 hours, and rotating speed is 200 ~ 220r/min; By ball milling good mixed slurry as in loft drier 120 ℃ dry 8 hours; Compound after drying is placed in to the agate tank and grinds, the compound after grinding is crossed to 120 mesh standard sieves; Compound after sieving is put into to corundum crucible, then be placed in after retort furnace is heated to 800-950 ℃ with the temperature rise rate of 3 ~ 5 ℃/min and be incubated 30 ~ 60min; Adopt melt pulling method that the melt-mixed material after insulation is placed in to deionized water fast, obtain original Li-- 2o-B 2o 3-SiO 2frit; Using the pristine glass material that obtains respectively by weight 180 ~ 200% and 150 ~ 160% add zirconia ball and dehydrated alcohol as ball-milling additive, ball milling 60 ~ 90min on Quick ball grinder, carry out fragmentation, rotating speed is 1200r/min; By ball milling good glass paste as in loft drier 120 ℃ dry 8 hours; Frit after drying is placed in to the agate tank and grinds, the compound after grinding is crossed to 200 mesh standard sieves, obtain uniform Li-- 2o-B 2o 3-SiO 2sintering aid;
In step 2, the calcium zirconate base-material that is 100% at weight part, add 3 ~ 12% the Li--that accounts for calcium zirconate base-material gross weight 2o-B 2o 3-SiO 2sintering aid, put into nylon ball grinder, by 180 ~ 200% and 150 ~ 160% of calcium zirconate base-material weight, adds zirconia ball and dehydrated alcohol as ball-milling additive respectively, and in planetary ball mill, ball milling is 8 ~ 12 hours, and rotating speed is 200 ~ 220r/min; By ball milling, good mixed slurry is put into 120 ℃ of oven dry of loft drier 8 hours; Compound after drying is placed in to the agate tank and grinds, the compound after grinding is crossed to 120 mesh standard sieves, obtain uniform CaZrO 3ceramic powder; To in the ceramic powder obtained, add the polyvinyl alcohol that weight percent is 6 ~ 8% to carry out granulation as tackiness agent, cross 60 ~ 80 orders; With tabletting machine compression moulding, be green compact again; The green compact of compression moulding, in 800 ℃ ~ 950 ℃ sintering, are incubated to 2 ~ 4 hours, make CaZrO 3microwave-medium ceramics.
Testing method of the present invention and test set are as follows:
1. the diameter of sample and thickness are used milscale to be measured;
2. measure resonant frequency and the quality factor of 20 ~ 80 ℃ by Agilent N5230C-220 vector network analyzer and the high low temperature experimental box of DWB2-6;
3. adopt Resonant-cavity Method to measure the quality factor of prepared cylindrical ceramic sample, the survey frequency scope is in the 6-8GHz scope.
The test result of specific embodiment of the invention microwave dielectric property refers to following table:
Figure DEST_PATH_IMAGE004

Claims (5)

1. a method that reduces calcium zirconate microwave-medium ceramics sintering temperature is characterized in that: step 1,
Li 2o-B 2o 3-SiO 2the preparation of sintering aid, Li 2o, B 2o 3, SiO 2make compound, put into nylon ball grinder, press respectively Li 2o-B 2o 3-SiO 2180 ~ 200% and 150 ~ 160% of compound weight adds zirconia ball and deionized water as ball-milling additive, and in planetary ball mill, ball milling is 8 ~ 12 hours, and rotating speed is 200 ~ 220r/min; By ball milling good mixed slurry as in loft drier 120 ℃ dry 8 hours; Compound after drying is placed in to the agate tank and grinds, the compound after grinding is crossed to 120 mesh standard sieves; Compound after sieving is put into to corundum crucible, then be placed in after retort furnace is heated to 800-950 ℃ with the temperature rise rate of 3 ~ 5 ℃/min and be incubated 30 ~ 60min; Adopt melt pulling method that the melt-mixed material after insulation is placed in to deionized water fast, obtain original Li 2o-B 2o 3-SiO 2frit; Using the pristine glass material that obtains respectively by weight 180 ~ 200% and 150 ~ 160% add zirconia ball and dehydrated alcohol as ball-milling additive, ball milling 60 ~ 90min on Quick ball grinder, carry out fragmentation, rotating speed is 1200r/min; By ball milling good glass paste as in loft drier 120 ℃ dry 8 hours; Frit after drying is placed in to the agate tank and grinds, the compound after grinding is crossed to 200 mesh standard sieves, obtain uniform Li 2o-B 2o 3-SiO 2sintering aid;
In step 2, the calcium zirconate base-material that is 100% at weight part, add Li 2o-B 2o 3-SiO 2sintering aid, put into nylon ball grinder, by 180 ~ 200% and 150 ~ 160% of calcium zirconate base-material weight, adds zirconia ball and dehydrated alcohol as ball-milling additive respectively, and in planetary ball mill, ball milling is 8 ~ 12 hours, and rotating speed is 200 ~ 220r/min; By ball milling, good mixed slurry is put into 120 ℃ of oven dry of loft drier 8 hours; Compound after drying is placed in to the agate tank and grinds, the compound after grinding is crossed to 120 mesh standard sieves, obtain uniform CaZrO 3ceramic powder; Be that 6 ~ 8% tackiness agents carry out granulation by adding weight percent in the ceramic powder obtained, cross 60 ~ 80 orders; With tabletting machine compression moulding, be green compact again; The green compact of compression moulding, in 800 ℃ ~ 950 ℃ sintering, are incubated to 2 ~ 4 hours, make CaZrO 3microwave-medium ceramics.
2. a kind of method that reduces calcium zirconate microwave-medium ceramics sintering temperature according to claim 1, is characterized in that: Li 2o, B 2o 3, SiO 2proportioning be 7:1:2.
3. a kind of method that reduces calcium zirconate microwave-medium ceramics sintering temperature according to claim 1 is characterized in that: in the calcium zirconate base-material that is 100% at weight part, add 3 ~ 12% the Li that accounts for calcium zirconate base-material gross weight 2o-B 2o 3-SiO 2sintering aid.
4. a kind of method that reduces calcium zirconate microwave-medium ceramics sintering temperature according to claim 1 is characterized in that: in the calcium zirconate base-material that is 100% at weight part, add 9% the Li that accounts for calcium zirconate base-material gross weight 2o-B 2o 3-SiO 2sintering aid.
5. a kind of method that reduces calcium zirconate microwave-medium ceramics sintering temperature according to claim 1, it is characterized in that: tackiness agent is polyvinyl alcohol.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104368819A (en) * 2014-10-16 2015-02-25 昆明理工大学 Method for preparing flake-shaped MWCNTs/Cu composite powder with small particle size
CN106747435A (en) * 2017-03-03 2017-05-31 河南科技大学 A kind of preparation method of the core shell structure microwave-medium ceramics of temperature stabilization
CN110156075A (en) * 2019-06-21 2019-08-23 安徽工业大学 It is a kind of to use sintering flue gas desulfurization ash low temperature preparation CaZrO3The method of powder
CN110194485A (en) * 2019-06-21 2019-09-03 安徽工业大学 It is a kind of to use sintering flue gas desulfurization ash low temperature preparation CaTiO3The method of powder

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
M.T.SEBASTIAN等: "Low loss dielectric materials for LTCC applications：a review", 《INTERNATIONAL MATERIALS REVIEWS》 *
WOO-JIN LEE等: "Decreasing of CaZrO3 sintering temperature with glass frit addition", 《CERAMICS INTERNATIONAL》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104368819A (en) * 2014-10-16 2015-02-25 昆明理工大学 Method for preparing flake-shaped MWCNTs/Cu composite powder with small particle size
CN106747435A (en) * 2017-03-03 2017-05-31 河南科技大学 A kind of preparation method of the core shell structure microwave-medium ceramics of temperature stabilization
CN110156075A (en) * 2019-06-21 2019-08-23 安徽工业大学 It is a kind of to use sintering flue gas desulfurization ash low temperature preparation CaZrO3The method of powder
CN110194485A (en) * 2019-06-21 2019-09-03 安徽工业大学 It is a kind of to use sintering flue gas desulfurization ash low temperature preparation CaTiO3The method of powder
CN110194485B (en) * 2019-06-21 2021-09-03 安徽工业大学 Low-temperature preparation of CaTiO by using sintered flue gas desulfurization ash3Method for producing powder
CN110156075B (en) * 2019-06-21 2021-09-10 安徽工业大学 Low-temperature preparation of CaZrO by using sintered flue gas desulfurization ash3Method for producing powder

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